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Electrolytic Iron

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Electrolytic Iron ELECTROLYTIC IRON ; DEPOSITED BY T H E COMMI T T E E O N (Brafcmate StuMes. 1 x ACC. No DATE ELECTROLYTIC IRON.. A STUDY OF THE PRODUCTION OF IRON BY ELECTROLYSIS, WITH SPECIAL REFERENCE TO ITS RECOVERY FROM SULPHIDE ORES.. THESIS Submitted by WILLIAM RAYMOND MoCLELLAND As Part of the Requirements for the Degree of Master of Soienoe. MAY L925. MoOILL UNIVERSITY, MONTREAL, CANADA. ELECTROLYTIC IRON. A Study of the Production of Iron by Electrolysis, with Special: Reference to its Recovery from Sulphide Ores.- PART I. Introduction Historical Outline and Descriptive* Physical Properties of Electrolytic Iron. PART II Theoretioal Considerations. A. Leaohing. B. Electrolysis. PART III. Experimental Research. A. Ore Body and Treatment of Ore. B. Leaching. C. Electro-deposition. General Summary and Conclusion. PART IV. Appendix. References. Sample Calculations. Bibliography. (1) PART I. INTRODUCTION. Iron, is the oommonest, most widely used, and at the same time the most vitally important of all the base metals. In the growth and developementr of modern civilization it assumes a dominant position.. Iron was not unknown to the anoients,nor were they unaware of its uses. As early as 1500 B.C.. the inhabitants of India; fashioned swords and spear heads. They even recognized, its qualities: for purpose* of construotion. Wrought1: iron beams measuring twenty feet in length have been found in the temple of Kanaruk dating from 1250 B.C. The metallurgy of iron at this period was extremely primative and continued so for many hundreds of year.s. It v;as notr until the sixteenth century that the introduction of-the air blast into the furnaoff made the progress of iron manufacture comparatively rapid.From thi'a period on, tha production increase-d. In US1* Henry Cort invented tha " puddling, process'1' for the manufacture of; wrought iron.. This was an advanoe step and greatly oheapenei the production of iron* In. the nineteenth century the famous researches and inventions of Sir Henry Bessemer, Sir William Siemens and others laid the foundation of the present day steel industry. The increasing demand for iron in all its numerous combinations has given impetus to the developementf of new metallurgical processes for its recovery.. The utilization of low grade ores and ores unsuitable for smelt­ ing has opened up further fields of. researoh and investigation. Coincident^with this increased demand for iron has been the depletion f of the world's supplies of fuel. This has to a small extent been ofset by the tremendous strides that have been made in the utilization of electrical energy during the last half oentury. (2). These facts have led many investigators to examine the possibilities of producing iron by eleetrical means. Two methods of recovery suggest themselvesJflrst, that of smelting where eleotrieity furnishes the required heat;: and seoond, by electrolysis from a solution obtained by leaching the ore. The first method is satisfaetorily employed in Sweden,1 where ohsap electric power, searoity of fuel, and high grade ore make such a process economically possible. The seoond method , that of electrolysis, has the advantage of producing a product of extreme purity and further ef utilizing ores whleh are not suitable for smelting; e.g. the sulphide ores of iron. Neither of the above methods can at the present time compete with the ordinary blast furnace. But for special purposes and under peculiar conditions they can add materially to the world1* supply of iron. It is the object of this thesis to investigate the problems of leaching pyrrhotite ore with ferrie chloride, and the production of iron by eleotrolysis of the resultant ferrous chloride solution The physioal properties of pure iron make it highly suitable for many metal products. Eleotrolytlo iron is used for boiler tubes, pipes in refrigeration machines, magnetic cores for electrical apparatus, use in alloys, eleotrioal transmission wires, etc. HISTORICAL OUTLINE AND DESCRIPTIVE. Eleotrolytlo iron has engaged the attention of investigators for many years. Probably the first to produce it was Bookbushmann in lffM-6. He deposited on a copper matrix a plate of iron 150 millimetres square and 2 millimetres thick. In 1&60 at Petrograd, the Russian chemist Klein succeeded in making blocks of eleotrolytlo iron. These were used as plateB for the printing of bank notes. The bath used was a solution containing 5 per cent of iron sulphate and 5 per oent of magnesium sulphate. The solution wan kept neutral by the (3) addition of magnesium carbonate. A low ourrent density was employed of 0.1 to 0.2 amperes per square decimetre. Feuquieres in 1S67 exhibited at Paris some galvanio deposits of iron, but his prooess was never divulged. The German firm of Merk in 1900 patented a prooess based on the elec­ trolysis of highly concentrated pure ferrous ohloride. A. ourrent density of J to ty amperes per square deoimetre was used and the solution was kept: at a 7 temperature of 70 C. Burgess and Hambueohen in 190*f produoed successfully quite a large quantity of electrolytic iron from a bath of a double sulphate of iron and ammonium. The temperature of their solution was kept constant at 50 0V and the ourrent density employed was 1.0 ampere per square deoimetre.- The* work was carried out in the laboratory of Applied Electrochemistry at the University of Wisconsin. Numerous trials were run using- a large number of eleotrolyfces, butr the double salt of ferrous ammonium sulphate was found to be the most satisfactory. The voltage was a little under 1.0 volt. The anodes were of wrought iron or steel and the cathodes of sheet iron with their surfaces carefully cleaned and smooth. From this series of investigations they found that the yield was about 2*2. lbs. per K.W. hour of 99.9^ pure iron. The deposited iron was very hard and had a very high melting point. Hydrogen was evolved on annealing from under 100 C. to a dull red heat. They consider that the hydrogen may be in the metal either as a hydride or simply as a condensed gas. Quantities of hydrogen to the extent of several hundred times the volume of the iron have been found. About the same time as the work of Burgess and Hambueohan,, Professor Foerster of Dresden carried out some investigations in this, oonneotion. The solution whioh he used was a slightly acid one of iron sulphate* It was keptr at a temperature of 95 C. andi a ourrent density of 2?«0 amperes per square decimetre. In 1907 Cowper-Colea patented a prooess employing, ai 20^ solution of sul^hocresylate of iron. Brisfly the prooess oonsists in leaching iron sorap or finely divided iron ora> with aoid» The leaching is aided by employing a small /o ourrent and using an insoluble anode materiad. The eleotnolytej used for the deposition cells oonsists of a 20$ solution, of: sulphooresylio acid saturated with iron. The iron, is deposited on revolving mandrels. These are coated with a thin deposit of lead. On the lead, the iron deposit oomes off in the form of a tube. The temperature of the solution is about 70 C. and the ourrent density: alxout 100 amperes per square foot. The solution.is kept oharged with iron oxide. No explanation is given for this, but the writer understands that a similar oondition is maintained in the cells at the works of the Company " Le Fer " , G-renoble,Franoe.. The reason given,is that a more satisfactory deposit is obtained,due to the oxide reducing the aci­ dity of the solution and further serving as a. meohanioal polisher to the depos- iting surfaoe.. Various German patents were granted in 1909; one of which specifies the use of highly concentrated solutions of iron ohloride and oaloiura ohloride. The temperature of these solutions was 110 C. with a ourrent density of 20 am­ peres per square decimetre. 1910 saw the first successful attempt to manufacture eleotrolytio iron on a commercial soaie.. The Company "'Le Fer" of Grenoble,Franoe. took out /3 patents for its manufacture. The prooess in principle oonsists of electrolysing a solution of neutral ferrous chloride and depositing the iron on cylindrical revolving cathodes. The anodes are of oast iron. The deposit is 99*97^ pure. It is first (5)* annealed to remove the occluded or combined hydrogen. The tubes are then turned. in a lathe, against a blunt tool whioh stretches and loosens the deposited; iron and it is then easily removed from the mandrel. These tubes are used as boiler tubes. They can be drawn tx> any required size. Dr. L. Guillet gives a comprehensive aocount of this prooess in the Journal of the Iron and Steel Institute, Vol- 90. 191^« The average composition of the iron after removal of the gases by annealing is as fellows:- Carbon. OJdQ^fi Silioon , . .0.X>07?o Sulphur <...0.006> Phosphorus O.OOff^. Iron 99.97^ By the aid of oertain operations and modifications ir* the electrolyte the phosphorus content was gradually reduced from 0.200$ in. 1911 to O.QOg^o in 191^. The pig iron used as anod9e has the following analysis:- Carbon ?v35^ Siliaon l*31/« Sulphur Q.QJfi Phosphorus. •..... 1.07/a A current density of 1000 amperes per square metre yields per kilo­ watt-year two tons of metal, inoluding cost of power for meohanical details of the plant , particularly the rotation of the cathodes*. The metal as deposited is extremely brittle due to the ocoluded be hydrogen. But by careful annealing this canAentirely removed and very duotile tubes obtained. The ourrent praotioe is to manufacture tubes of four metres in length, diameter of one to two hundred millimetres and with a tniokness of 0.1 to 6.0 millimetres* At the time this paper of Dr.
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